Process of recovering separating liquids from separated solids.



F. I. DU PONT. PROCESS OF REGOVERING SBPARATING LIQUIDS FROM SEPABAIBD SOLIDS.

APPLIOATION FILED JULY 15, 1910. 1,081,949, Patented Dec. 23, 1913.

Z SHEETS-SHEET 1.

IIWENTW? WITNESSES:- Mm/K as x 5y ,4 ,9 1

F. I. DU PONT.

PROCESS OF RECOVERING SEPARATING LIQUIDS FROM SEPARATED SOLIDS.

APPLICATION FILED JULY 15, 1910.

1,081,949, 7 Patented Dec. 23, 1913.

2 SHEETS-SHEET 2.

WITNESSES: "VF/V70 lit) said solids.

ll i' il. .l l l'llllilillllli COPY FMMGW ]I.- no roar, @li WELMING'TON, DELAWARE, ASBIGNOR Till INTERNATIONAL W611) GOMPANY, .& CORTQQEMEION Oh DELAWARE.

IPRQGMHW 69F {ENTERING BEPAMATIIXTG LIQUlIDS FROM EEJPARATED SOLIDS.

inane-an.

I llpeciflcation oi Letters Patent.

ratenteancc. as, rare.

To all whom it may concern:

Be it known that I, FRANCIS K. on Pour, a citizen of the United States, residing at Wilmington, county at Newcastle, and State of Delaware, have invented a new and useful improvement in Processes of Recovering Eleparating Liquids from Se arated Eiolids which the following is a nil, clear, an erect description, reference being had to the accompanyin drawings, which orm a part of this speci cation.

In the gravity separation of solids by means of a liquid, a certain amount of this liquid is carried off with the separated constituents. "Where such SBPiLI'dtlOIl liquid is other than water, it is in most cases too valuable to be lost and some means should be provided, if the'process is tobe carried on economically, to recover said liquid from.

the solids which carry it so that it ma be returned again to the separating vesse l have used certain bromide for such separating liquid, and in carrying out my investigation with respect to such separation by such liquids, I discovered that antimony bromid and tin bromid or a mixture of the two or such bromid liquid was soluble in alcohol, and therefore, by passing the mate rial carrying such separating liquid through the alcohol, I could dissolve out from t e solids the bromide which were carried by Further, as the volatilization temperature of the alcohol is considerably lower than that of the bromide, I could subject such solution to the action of heat-sufiicient to volatilize the alcohol but 'insufficient to volatilize the separating liquid. As a consequence, the separating liquid could be removed from the solids and its solvent,

then removed from it, leaving the gravity liqulid which could be then returned to the tan Therefore my invention broadly consists in recovering the separating liquld carried off by the separated material by subjecting the material to the action of a solvent of the separating liquid, and of lower volatilization temperature than the separating liqaid, and then volatilizing the solvent and recovering the separating liquid.

In carrying out this process, I carry on the process in the following manner. I use a tank which is air-tight and which is divided into liquid sections. The liquid is caused to circulate in this tank through the sections 1n one direction while the material carryin the separating liquid is caused to travel t rough said tank in the opposite direction. In this operation the liquid in the first section of the tank dissolves more of the gravit liquid from the material than the succee i'ng section, and this is true with respect to each. succeeding section. Therefore, it is necessary that the solvent liquid should be urer as the quantity of the gravity liquid in the separated material becomes less. It is "for this reason that I divide the tank into sections, and I provide each sec tion with a heating a paratus sufficient to volatilize 'the alcoho but insutiicient to volatilize the gravity liquid. The volatilized solvent from each section is carried to a condenser and returned to the tank at a section nearer the exit end for the solids of the tank or more remote from the liquid discharge end of the tank. This not only produces a condition of providing the purest alcohol nearest the oint of exit of the solids, and so gradu'a 1y down to the liquid discharge of tne tank, but also creates a flow of the liquid in the tank or section of the tank in a direction opposite to the travel of the solid material.

I will now describe the embodiments of my invention and then fully point out the invention in the claims.

In the drawings Figures 1 and 2 are side elevations, partly in section, of an apparatus embodying my invention and adapted to carry out my process. a is a chute into which the separated ma terial from the gravity separator asses. This chute enters the tank I), Whic is a closed tank and divided into liquid sections by the partitions o. In this tank is a conveyer d driven by the gear f. In this tank is a liquid 9 which, if the gravity liquid be a bromid, is alcohol.

h, h, It, h, are heaters, one for each section of the tank. The heat applied to each section is such as to volatilize the solvent liquid but is less than that necessary to v01- at-llize the separating liquid.

At the right hand end of the tank is an upwardly inclined portion '5 in which is a conveyor j having, with the conveyer d, the

driving connection k. Each section of the tank has a pi e Z in connection with a condenser m, an a pipe a, an outlet from said condenser m. The pipe it enters the tank 6, at a succeeding section from that which the pipe Z, leading to the corresponding con denser m, opens. At the end of the upwardly inclined portion a is the chute or channel 0 leading to the seconda tank which contains water or a liqui and 1s provided with a heater 9. From this tank leads the pipe r to the rectifier 3 provided with the drip pipe t. From the rectifier the pipe it leads to the analyzer 'v, the lower portion of which is connected by the ipe to with the rectifier s, A pipe as leads rom the upper part of the analyzer 'v to the.

condenser 1 and z is a return pipe for the condensed vapors and leading to an opening into the upwardly inclined portion 6. Connected to the upwardly inclined portion a of the bank is the pipe 21 leading to the condenser 2, provided with the return pipe 3 leading back to the liquid in the tank 6."

5 is the liquid outlet from the tank 5, which leads to the receiving vessel 6 which is jacketed by the jacket 7. From this receiving vessel 6 a pipe 8 leads to the condenser 9, from which a return pipe 10 leads to the first section of the tank I). From the lower portion of the vessel 6 a pipe 11 leads to the pump 12 from which a ipe 13 leads back to the separating device lnot shown).

The operation is as follows: The separated material carrying some of the separating liquid,say a bromid, passes down the chute or channel a, into the tank 6 where it is caught by the conveyer d and caused to travel from left to right in the sections of the tank. Tn the first section, the material containing at that point the greatest amount of the separating liquid, a large quantity will be readily dissolved by the alcohol which is the liquid in the tank. This is true'in degree with respect to all of the sections. vaporize the alcohol, causing it to pass through the condenser m and return to the next forward section (in the direction of movement of the solid material). In this way there will be a constant flow of the alcohol in a reverse direction to the move' ment of the solids so that practically the first movement of the alcohol when it is in the purest condition will be upon the ma terial' at the time in which it carries the least amount of the gravity liquid, which is, of course, desirable, and the alcohol will heslightly less pure in the next case where there is less action, and so on to the outlet pipe 5, or the section nearest the outlet pipe, which section will contain all or practically all or the solvent in the separated The heater h in each section will which in this case, as stated, is alcohol,-

which boils at 78 C. However, as the liquid in the bath becomes more contaminated as it passes to the liquid discharge end in the direction of the current, the actual temperature will vary, increasing in temperature in the direction of the current liquid flow. Thus the initial heater in the direction of the currentflow of the liquid should be at least 78 degrees, the temperature of the next heater should be at least in excess of 78 degrees, suficient to keep the liquid boiling. This follows all the way through. In fine, the temperature of each of the heaters should be such as at least to boil the liquid at the point where the heat is applied. Of course, I do not intend to limit myself to the entry of this pipe into the particular section as shown, as it may be caused to enter any one of the sections desired. The gravity liquid will pass out from the vessel 6 through the pipe 11 into the pump 12, from which it will be pumped through the pipe 13 back to the separatlng vessel,

It may be noted that the volatilized product carried by the right hand pipe Z, passing into its condenser m, will return into the wing, but it will be seen that it returns into the wing at the level of the liquid in the tank 6, thereafter passing into the liquid of that tank In order to recover from the solids any alcohol which may be carried by them, I provide in the upwardly inclined portion the heating jacket 19, the pipe 21 and the condenser 2 and return pipe 3, which return pipe 3 enters the pipe n, of the righthand condenser m, and thus the alcohol is delivered again into the liquid of the tank.

In the vessel or tank ,2) is, as stated, water and the solids passing down the chute 0 will pass into this water, which will remove any final trace of alcohol, which final trace, by the heater 9, will be volatilized, pass up through the rectifier 8, through analyzer v and into a condenser y, from which, through pipe 2, it will be returned to the liquid in the tank b. Finally, the tankp has an inclined wing it with the conveyer 15 operatively connected by universal joint 16 with theconveyer 17, and flows into the chute 18 through which it may be carried to the desired'point Having now fully described my invention,

them in a liquid of higher volatilizin point than the washin liquid, and maintalned at a temperature a ove the volatilizing point of said washing liquid, and recovering by condensation the washing liquid.

9. The hereinbefore mentioned method of recovering the liquid used in gravity liquid se aration, which consists in washing the solids in a liquid more volatile than the separating liquid and in which said liquid is soluble, removing the washed solids from the washing liquid and subjecting them to heat suficient to drive ofi the ma or portion of the washing liquid, and finally immersing them in a liquid of higher volatilizing point than the washing liquid, and maintalned at a temperature ove the volatilizing point of said washing liquid, and recovering by condensation the washing liquid, and separating by distillation of the washings the washing li uid from the separating liqu1d.

10. The ereinbefore 'mentioned method of recovering a liquid soluble in alcohol used in gravity liquid separation of solids, which consists in washing the solids after separation in alcohol, removing them from the alcohol and subjecting them to heat suficient to volatilize the major portion of the alcohol and finally immersin them in boiling water,

condensing the alco ol driven 0d and by means of a rectifying system recovering the last traces of alcohol from the vapors of the boiling water.

11. The hereinbefore mentioned method of recovering a liquid soluble in alcohol used in gravity liquid separation of solids, which consists in washing the solids after separation in alcohol, removingthem from the alcohol and subjecting them to heat suficient to volatilize the major portion of the alcohol 4 and finally immersing them in boiling water, condensing the alco ol driven ed and by i eaneae means of a rectifying system recovering the last traces of alcohol from the vapors of the boiling water, and separating by distillation the alcohol from the separating 1i uid.

12. The hereinbefore mentione method of recovering the liquid used. in gravity liquid separation, which consists in washing the solids in a liquid more volatile than the separating; liquid and in which said liquid is soluble, removing the washed solids from the washing liquid, and subjecting them to heat suficient to drive 0d the major portion of the washing liquid, and finally immersing them in a liquid of higher volatllizin point than the washin liquid, and maintained at a temperature a ove the volatilizing point of said, washing liquid, and recovering by condensation the washing liquid 13. The hereinbefore mentioned method of recovering the liquid used in gravity liquid separation, which consists in washing the solids in a liquid more volatile than the separating liquid, and in whichsaid liquid is soluble, removing the washed solids from the washing liquid and subjecting them to heat suliicient to drive 0d the major portion of the washing liquid, and finally immersing them in a liquid of higher volatilizin point than the washin liquid, and maintained at a tem erature a ove the volatilizing point of sai washing liquid, recovering by con densation the washing liquid, and separating by distillation of the washings the washing hquid from the separation liquid.

In testimony of which invention, T have hereunto set my hand, at Philadelphia, on this 8th day of July, 1910.

CTS l; on PUNT. 

